EP3051287B1 - Dispositif d'analyse et procédé d'analyse - Google Patents

Dispositif d'analyse et procédé d'analyse Download PDF

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Publication number
EP3051287B1
EP3051287B1 EP14847785.4A EP14847785A EP3051287B1 EP 3051287 B1 EP3051287 B1 EP 3051287B1 EP 14847785 A EP14847785 A EP 14847785A EP 3051287 B1 EP3051287 B1 EP 3051287B1
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EP
European Patent Office
Prior art keywords
sample
flow path
gas
heating
laser light
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Application number
EP14847785.4A
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German (de)
English (en)
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EP3051287A4 (fr
EP3051287A1 (fr
Inventor
Yasushi Hirata
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Horiba Ltd
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Horiba Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44—Sample treatment involving radiation, e.g. heat
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
    • G01N33/004—CO or CO2
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
    • G01N33/0042—SO2 or SO3
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/02—Induction heating
    • H05B6/22—Furnaces without an endless core
    • H05B6/24—Crucible furnaces

Definitions

  • the present invention relates to an analysis device such as an elemental analyzer or the like that analyzes elements such as carbon (C) and sulfur (S) that are contained in a sample of, for example, steel, a non-ferrous metal, or a ceramic or the like, and to an analysis method.
  • an analysis device such as an elemental analyzer or the like that analyzes elements such as carbon (C) and sulfur (S) that are contained in a sample of, for example, steel, a non-ferrous metal, or a ceramic or the like, and to an analysis method.
  • Patent document 1 a combustion improver is used in the above-described elemental analyzer in order to accelerate the combustion of the sample.
  • Non-patent document 1 discloses an open-path laser-induced plasma spectrometer (OP-LIPS) attached to an induction furnace for the analysis of steel.
  • OP-LIPS laser-induced plasma spectrometer
  • Patent document 1 Japanese Patent Application JP2000266741 A
  • Non-patent document 1 S. PALANCO ET AL: "Analytical control of liquid steel in an induction melting furnace using a remote laser induced plasma spectrometer", JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, vol. 19, no. 4, 23 March 2004 (2004-03-23), page 462, XP055352755,ISSN: 0267-9477, DOI: 10.1039/b400354c [Disclosure of the Invention]
  • tungsten which is a rare metal, is contained in the combustion improver, so that, if a combustion improver is used, the additional problem arises that the running costs incurred by the analysis become expensive.
  • the present invention was conceived in order to solve the above-described problems, and it is a principal object thereof to make it possible to efficiently heat and combust a sample without using a combustion improver.
  • the analysis device is an analysis device that heats a sample inside a sample holding portion, and analyzes the gas that is thereby generated, and that is provided with: an induced current generating mechanism that generates by electromagnetic induction an induced current in the sample; and a laser irradiation mechanism that irradiates laser light onto the sample, and the induced current generating mechanism and the laser irradiation mechanism are made to act simultaneously on the sample.
  • the analysis method according to the present invention is an analysis method in which a sample is heated inside a sample holding portion, and the resulting gas that is thereby generated is analyzed, wherein the sample is heated by the induced current generating mechanism, which generates an induced current in the sample by electromagnetic induction, and by the laser irradiation mechanism, which irradiates laser light onto the sample, acting simultaneously on the sample.
  • the analysis device prefferably be further provided with a flow path forming component in which a supply flow path that supplies oxygen into the interior of the sample holding portion is formed, and for a transmission window that allows to transmit laser light to be formed in the flow path forming component, and for an optical path of the laser light that has been transmitted through the transmission window to be formed inside the supply flow path along with the flow path direction of the supply flow path.
  • the supply flow path prefferably has a rectilinear flow path having one end that opens in the direction of the sample, and having the transmission window formed in the other end thereof.
  • the laser light is irradiated along a rectilinear flow path onto the sample, the laser light that has passed through the transmission window can be guided directly onto the sample through the transmission window without any optical components such as mirrors being used.
  • An elemental analyzer 100 heats and combusts a sample X which is made, for example, from metal or the like, and analyzes elements such as carbon (C) and sulfur (S) and the like that are contained in the sample X from the gas that is thereby generated.
  • this elemental analyzer 100 is equipped with a heating furnace 2 which is a sample housing portion in which a crucible 1 that holds the sample X is placed, a gas analyzer 3 that analyzes the gas generated by the combustion of the sample X, an oxygen supply mechanism 4 that supplies oxygen to the interior of the heating furnace 2, an induced current generating mechanism (induction heating mechanism) 5 that generates an induced current in the sample X inside the crucible 1 via electromagnetic induction so that the sample X is induction heated, a laser irradiation mechanism (laser heating mechanism) 6 that heats the sample X by irradiating laser light onto the sample X, and a control unit 7 that controls operations of the oxygen supply mechanism 4, the induction heating mechanism 5, and the laser heating mechanism 6.
  • a heating furnace 2 which is a sample housing portion in which a crucible 1 that holds the sample X is placed
  • a gas analyzer 3 that analyzes the gas generated by the combustion of the sample X
  • an oxygen supply mechanism 4 that supplies oxygen to the interior of the
  • the crucible 1 is mounted on a placement stand 8 while internally holding the sample X.
  • the crucible 1 is formed, for example, by a magnetic body such as a ceramic material or the like that has a conductive heating element.
  • the placement stand 8 is constructed such that it can be moved up and down by a cylinder mechanism (not shown) between a heating position where the sample X inside the crucible 1 is heated inside the heating furnace 2, and a removal position where the crucible 1 is mounted on or removed from the placement stand 8.
  • the heating furnace 2 is constructed such that it heats the sample X that it is holding internally, and then guides the gas that is thereby generated to the gas analyzer 3.
  • the heating furnace 2 is provided with a substantially cylinder-shaped furnace main body 21, a gas outflow path 22 that is formed in a side wall 211 of the furnace main body 21 and guides the gas to the gas analyzer 3, and a filter 23 that is provided so as to extend around the inner circumference of the side wall 211 inside the furnace main body 21.
  • the filter 23 of the present embodiment is provided slightly apart from an intake port 221 of the gas outflow path 22 in the direction of the pipe axis of the furnace main body 21, and the gas generated as a result of the sample X being combusted inside the crucible 1 flows into the gas outflow path 22 via this filter 23.
  • the gas analyzer 3 analyzes the gas that is guided into the gas analyzer 3 through the gas outflow path 22, and thereby determines the content of each component contained in the sample X.
  • the gas analyzer 3 performs this analysis by employing, for example, a non-dispersive infrared absorption method (NDIR method).
  • NDIR method non-dispersive infrared absorption method
  • this gas analyzer 3 has a non-dispersive infrared detector (not shown) and determines the content of carbon (C) and sulfur (S) and the like contained in the sample X by detecting CO 2 , CO, SO 2 , and the like that are contained in the gas.
  • the oxygen supply mechanism 4 supplies oxygen to the interior of the heating furnace 2.
  • the oxygen supply mechanism 4 is equipped with a flow path forming component 41 in which a supply flow path L that supplies oxygen to the interior of the heating furnace 2 is formed, and with an oxygen cylinder which serves as an oxygen supply source 42 that is used to feed oxygen to the supply flow path L.
  • the flow path forming component 41 is a substantially block-shaped component, and is mounted such that it penetrates a top surface 212 of the heating furnace 2 in order to supply the oxygen flowing along the supply flow path L to the interior of the heating furnace 2. Furthermore, a transmission window 411 that transmits laser light is formed in the flow path forming component 41 of the present embodiment, and this transmission window 411 is in the form of a transparent, flat plate in the present embodiment.
  • the supply flow path L has a rectilinear first flow path L1 and a, for example, rectilinear second flow path L2.
  • One end of the first flow path L1 opens in the direction of the sample X inside the crucible 1, while the transmission window 411 is formed in the other end of the first flow path L1.
  • One end of the second flow path L2 connects to the other end of the first flow path L1, while an inlet port 41b through which oxygen is introduced from the oxygen supply source 42 is formed in the other end of the second flow path L2.
  • the transmission window 411 is formed on the opposite side from an aperture 41a in the first flow path L1, and the transmission window 411, the aperture 41a, and the sample X inside the crucible 1 are positioned on a straight line.
  • the second flow path L2 is formed perpendicularly to the first flow path L1. Oxygen supplied from the oxygen supply source 42 firstly passes through this second flow path L2 before flowing through the first flow path L1, and is then blown directly onto the sample X via the aperture 41a in the first flow path L1.
  • the above-described flow path forming component 41 is formed such that it is able to be moved by a drive unit (not shown) in a direction that is parallel to the flow path direction of the first flow path L1. As a result, it is possible to adjust the height of the aperture 41a of the first flow path L1 inside the heating furnace 2.
  • a cleaning body such as a brush or the like (not shown) is provided on an outer side surface of the flow path forming component 41. Inner surfaces of the filter 23 and the heating furnace 2 can be cleaned by this cleaning body as a result of the flow path forming component 41 being moved by the drive unit.
  • the induction heating mechanism 5 is an induced current generating mechanism that generates an induced current in the sample X held in the crucible 1 by means of high-frequency induction heating.
  • the induction heating mechanism 5 is equipped with a coil 51, and a power supply 52 that applies high-frequency AC voltage to the coil 51.
  • the coil 51 is provided around the outer circumference of the furnace main body 21, and the height of the placement stand 8 is set such that the crucible 1 is positioned on the inside of the coil 51 when the high-frequency AC voltage is being applied to the coil 51.
  • conductive heat-generating elements contained in the crucible 1 are made to generate heat by the high-frequency induction heating so that the sample X inside the crucible 1 is heated.
  • the laser heating mechanism 6 is a laser irradiation mechanism that irradiates laser light onto the sample X.
  • the laser heating mechanism 6 is equipped with a laser light source 61 that emits laser light.
  • the laser light source 61 of the present embodiment is located above the furnace main body 21, and emits laser light perpendicularly towards the transmission window 411 of the above-described flow path forming component 41.
  • an optical path B of the laser light transmitted through the transmission window 411 is formed inside the supply flow path L and parallel with the flow direction of the supply flow path L.
  • laser light that has passed through the transmission window 411 is transmitted in the flow direction along the first flow path L1. This laser light then travels from the aperture 41a through the interior of the heating furnace 2 towards the sample X, and is irradiated directly onto the sample X.
  • a semiconductor laser that provides an output of between 45W and 200W is used for the laser light source 61.
  • control unit 7 is an electrical circuit formed by, for example, a CPU, internal memory, and an AD converter and the like.
  • the control unit 7 functions as an oxygen supply control unit 71, an induction heating control unit 72, and a laser heating control unit 73.
  • the oxygen supply control unit 71 adjusts the pressure or the flow rate of the oxygen that is supplied from the oxygen supply source 42 to the interior of the heating furnace 2 via the supply flow path L by transmitting a signal to the oxygen supply source 42.
  • the induction heating control unit 72 adjusts the output of the high-frequency AC voltage applied by the power supply 52 to the coil 51 by transmitting a signal to the power supply 52.
  • the laser heating control unit 73 adjusts the output of the laser light emitted by the laser light source 61 by transmitting a signal to the laser light source 61.
  • the induction heating control unit 72 and the laser heating control unit 73 control the induction heating mechanism 5 and the laser heating mechanism 6 such that the respective heating mechanisms 5 and 6 act simultaneously to heat the sample X. In other words, they perform control such that a state in which the induction heating mechanism 5 supplies an induced current to the sample X and a state in which the laser heating mechanism 6 irradiates laser light onto the sample X are generated simultaneously. More specifically, the induction heating control unit 72 and the laser heating control unit 73 control the respective heating mechanisms 5 and 6 such that a state in which the sample X is heated simultaneously by the induction heating mechanism 5 and the laser heating mechanism 6 continues for a predetermined length of time.
  • the induction heating control unit 72 transmits a signal to the power supply 52 at the same time as the laser heating control unit 73 transmits a signal to the laser light source 61.
  • the induction heating control unit 72 controls the power supply 52 such that the high-frequency AC voltage is supplied continuously from the power supply 52 to the coil 51, for example, for 30 seconds, while the laser heating control unit 73 controls the controls the laser light source 61 such that the laser light is irradiated continuously from the laser light source 61 onto the sample X, for example, for 30 seconds.
  • the sample X is heated simultaneously by the induction heating mechanism 5 and the laser heating mechanism 6 for a period of 30 seconds.
  • the length of this heating period is not limited to 30 seconds and can be set to a desired time depending on the sample X.
  • the induction heating mechanism 5 and the laser heating mechanism 6 simultaneously heat the sample X, it is possible to efficiently heat the sample X and thereby accelerate the combustion thereof. Moreover, it is not necessary for a combustion improver to be used. Because there is no need to use a combustion improver, no dust that is created by the combustion improver is generated. Accordingly, there is no need for a dust suction mechanism to be provided, and no measurement errors that are caused by gas adhering to the dust are generated.
  • the existing supply flow path L is able to also function as the optical path B of the laser light. Accordingly, there is no need to create a complicated structure to irradiate laser light onto the sample X.
  • the transmission window 411 is formed on the first flow path L1 on the opposite side from the aperture 41a, and oxygen is supplied through this aperture 41a into the interior of the heating furnace 2, it is possible to prevent soot and the like that is inside the heating furnace 2 from flowing back along the first flow path L1 and becoming adhered to the transmission window 411.
  • a drive unit (not shown) is able to adjust the height of the aperture 41a of the first flow path L1 inside the heating furnace 2 by moving the flow path forming component 41, it is possible to place the sample X in the optimum state of combustion by controlling the speed at which oxygen is supplied to the sample X.
  • the induction heating mechanism and the laser heating mechanism transmit signals simultaneously to the power supply and the laser light source respectively, however, it is not absolutely essential for these signals to be transmitted simultaneously, and it is also possible for the signals to be transmitted after predetermined time intervals. Namely, provided that there is a period in which the heating by the induction heating mechanism and the heating by the laser heating mechanism are performed simultaneously, then it is acceptable for the start times of the heatings performed by the respective mechanisms to be mutually different, and for the end times of these heatings to also be mutually different.
  • the transmission window is formed on the opposite side from the aperture on the first flow path, however, as is shown in FIG. 3 , it is also possible, for example, for the transmission window 411 to be formed on the opposite side from the oxygen supply source 42 on the second flow path L2, and for the laser light that has passed through the transmission window 411, for example, to be reflected by an optical component such as a reflection mirror 62 or the like such that it is irradiated onto the sample X.
  • the coil is provided around the outer circumference of the furnace main body, however, it is also possible for the coil to be provided, for example in the bottom portion of the crucible, or on the top surface of the placement stand.
  • a carrier gas into the interior of the heating furnace from underneath the heating furnace in order to enable the gas that is combusted inside the crucible to flow efficiently along the gas outflow path.
  • a gas that contains oxygen may be used for this type of carrier gas.
  • the supply flow path L of the above-described embodiment is used to supply oxygen to the interior of the sample holding portion, however, it is also possible to employ a structure in which the supply flow path L supplies another gas (which may be an oxygen-containing gas) to the interior of the sample holding portion, and the laser light is irradiated onto the sample after being transmitted through this supply flow path L.
  • the supply flow path L supplies another gas (which may be an oxygen-containing gas) to the interior of the sample holding portion, and the laser light is irradiated onto the sample after being transmitted through this second supply flow path.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Combustion & Propulsion (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Molecular Biology (AREA)
  • Electromagnetism (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Waste-Gas Treatment And Other Accessory Devices For Furnaces (AREA)
  • Muffle Furnaces And Rotary Kilns (AREA)
  • General Induction Heating (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Sampling And Sample Adjustment (AREA)

Claims (4)

  1. Dispositif d'analyse (100) pour chauffer et brûler un échantillon, et pour analyser du gaz qui est généré par chauffage et combustion de l'échantillon, le dispositif d'analyse (100) comprenant :
    un analyseur de gaz (3) pour analyser le gaz ;
    un foyer de chauffage (2) pour contenir l'échantillon ;
    un mécanisme générateur de courant induit (5) pour générer par induction électromagnétique un courant induit dans l'échantillon ; et
    un mécanisme de rayonnement laser (6) pour émettre une lumière laser vers l'échantillon, dans lequel
    le mécanisme générateur de courant induit (5) et le mécanisme de projection de laser (6) sont configurés pour agir simultanément sur l'échantillon afin de chauffer l'échantillon pour une combustion accélérée de l'échantillon, et afin de générer le gaz à analyser ;
    le foyer de chauffage (2) comprend une trajectoire d'écoulement de gaz (22) qui est configurée pour guider le gaz généré vers l'analyseur de gaz (3).
  2. Dispositif d'analyse (100) selon la revendication 1, comprenant en outre
    un composant formant trajectoire d'écoulement (4) pour former une trajectoire d'écoulement d'alimentation qui alimente le foyer de chauffage (2) en oxygène, dans lequel
    une fenêtre de transmission (411) qui permet de transmettre la lumière laser est formée dans le composant formant trajectoire d'écoulement (4), et une trajectoire optique de la lumière laser qui a été transmise à travers la fenêtre de transmission (411) est formée à l'intérieur de la trajectoire d'écoulement d'alimentation avec la direction de trajectoire d'écoulement de la trajectoire d'écoulement d'alimentation.
  3. Dispositif d'analyse (100) selon la revendication 2, dans lequel la trajectoire d'écoulement d'alimentation a une trajectoire d'écoulement rectiligne ayant une extrémité qui s'ouvre en direction de l'échantillon, et ayant la fenêtre de transmission (411) formée dans son autre extrémité.
  4. Procédé d'analyse pour chauffer et brûler un échantillon à l'intérieur d'un foyer de chauffage (2), et pour analyser le gaz résultant qui est généré par chauffage et combustion de l'échantillon, le procédé d'analyse comprenant :
    le chauffage de l'échantillon qui est contenu dans le foyer de chauffage (2) avec un mécanisme générateur de courant induit (5), qui génère un courant induit dans l'échantillon par induction électromagnétique, et par un mécanisme de rayonnement laser (6), qui émet une lumière laser vers l'échantillon, agissant simultanément sur l'échantillon afin de chauffer l'échantillon pour une combustion accélérée de l'échantillon, et afin de générer le gaz à analyser ;
    le guidage du gaz généré, par une trajectoire d'écoulement de gaz (22) vers un analyseur de gaz (3) ; et
    l'analyse du gaz dans l'analyseur de gaz (3).
EP14847785.4A 2013-09-25 2014-09-10 Dispositif d'analyse et procédé d'analyse Active EP3051287B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2013198729 2013-09-25
PCT/JP2014/073903 WO2015045869A1 (fr) 2013-09-25 2014-09-10 Dispositif d'analyse et procédé d'analyse

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EP3051287A1 EP3051287A1 (fr) 2016-08-03
EP3051287A4 EP3051287A4 (fr) 2017-04-19
EP3051287B1 true EP3051287B1 (fr) 2020-08-05

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US (1) US9606090B2 (fr)
EP (1) EP3051287B1 (fr)
JP (1) JP6494517B2 (fr)
CN (2) CN105556303A (fr)
WO (1) WO2015045869A1 (fr)

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US10627355B2 (en) 2015-12-07 2020-04-21 Horiba, Ltd. Analysis device
KR20170093637A (ko) * 2016-02-05 2017-08-16 한국전자통신연구원 이종 네트워크 환경에서 미디어 전송 스트림 버퍼링 방법 및 이를 이용한 영상 수신 장치
CN109254108B (zh) * 2017-07-12 2023-02-17 株式会社堀场制作所 分析装置和分析方法
CN108593416B (zh) * 2018-04-08 2020-09-08 国家纳米科学中心 微纳粒子检测系统及方法
DE102018207165A1 (de) * 2018-05-08 2019-11-14 GEOMAR Helmholtz Centre for Ocean Research Kiel Vorrichtung zum Behandeln von Proben für eine quantitative Elementaranalyse bezüglich C, N und/oder S sowie Zufuhreinrichtung, Verwendung, System und Verfahren
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CN111537669A (zh) 2020-08-14
EP3051287A4 (fr) 2017-04-19
JP6494517B2 (ja) 2019-04-03
CN105556303A (zh) 2016-05-04
WO2015045869A1 (fr) 2015-04-02
JPWO2015045869A1 (ja) 2017-03-09
US9606090B2 (en) 2017-03-28
US20160231298A1 (en) 2016-08-11
EP3051287A1 (fr) 2016-08-03

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